Penetrometer and filling device therefor for porosimeters



Jan. 15, 1963 w. c. HAMPTON 3,073,357

PENETROMETER AND FILLING DEVICE- THEREFOR FOR POROSIMETERS Flled May 12,1958 2 Sheets-Sheet 1 To Ilia/0M Pu MP MERtl/RY Barns INVENTOR. WILL/AMC. HAMPTON WZM' Arm #2 NE Y Jan. 15, 1963 w. c. HAMPTON 3,073,357PENETROMETER AND FILLING DEVICE THEREFOR FOR POROSIMETERS 2 Sheets-Sheet2 Filed May 12, 1958 FI'E.4-

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Arrolz NE Y test. Tlivoluuie ofpenetrati n This invention relates toporosimeters, and more particularly to a penetrometer and a fillnigdevice there for for use with a porosimeter of the-type employing themercury intrusion method.

I United States Patent A main object of the invention is to provide anovel 7 and improved penetrometer and a filling device therefor for usein a porosimeter of the type employing the mercury intrusion method tomeasure the sizes and volumes of the pores of porous materials.

A further object of the invention is to provide an improved penetrometerfor use in a porosimeter, said penetrometer being simple inconstruction, being easy to fill, and which is especially suitable foruse in testing powdered samples of material, the penetrometer beingformed and arranged so that it is not necesasry to employ means to plugup its capillary stem to prevent the powdered material from entering thecapillary passage thereof and 1 so that the inconvenience and inaccuracyinvolved in using such means is avoided.

A still further object of the invention is to provide an improvedpenetrometer and filling device therefonfor use in a porosimeter of thetype disclosed in US. Patent No;

1 2,886,964 to Justin I. Shapiro and'Nathaniel M. Winslow;

A still further object of the invention is to provide animprovedfillingldevice' for a penetrometer for use in a porosimeter' ofthe typ'e employing the mercury intrusion method, such as is disclosedinUS. Patent No. 2,886,964,

said filling devicebeing arranged so that itis possible to always readthe low valued" end of the penetrometer scale while the penetrometeris-installed in its invertedf position in the filling device, and beingfurther arranged so that the pressuresin the lower portions ofthe-filling 5 7 device are, constantly equalized, whereby 'accurateporosity data at the large pore end'of the porosity spectrum of a sampleunder test maybe obtained.

Further objects and advantages of the invention willbecome apparent,from the,;following description and 7 claims, and from theaceompanying' drawings, whereinf FIGURE l is a side elevatiohalview,}partly"in vertical cross-section, of, an improved penetrometerand-"a filling device therefore, constructed in accordance withthepres-- 'ent invention, the' penetrometer being shown in its invertedposition andarranged for filling. y i g Y FIGURE ,2 is a horizontal"cross-sectional view taken on line 2+2 of.FIGURE 1. 4 I

FIGURE 3 is an enlarged vertical cross-sectional view taken through thebulbend of the p'enetrometer. Oil-11 in 3i.of.FIGURE,1.

- -Q+IFIGURE 4i'isia horizontal cross-sectional view-taken 2 bittheline4- 4of FIGURE 3.

, FIGURE 5. isfa;schematic view showinglthe' conduit connections ofressureiin said prespre vessel and containing th' shown in FIGURE 1.

Patented Jan. 15, 1963 ice cation of pressure, at each pressure, is readon the cali-' brated stem of the penetrometer, which is visible througha transparent Window section of the pressure vessel.

The porosimeter includes respective pressure gauges 21,

"32 through a cross fitting 36. A hydraulic fluid supply conduit 34,provided with a manually controlled valve 28 is connected between afluid reservoir and the pressure generator 24. Gauge 23 is connectedthrough a conventional gauge protector 38 and a conduit 39 to crossfitting 36. 7

Gauge 22 is connected through a conventional gauge protector 40 and aconduit 41, including a manually controlled cutofi valve 42, to thecross fitting '36.

Gauge 21 is connectedthrough a conduit 44- and a vacuum cut-off valve45'to a conventional external vacuum pump. Also connected to the conduit44 is a conduit 47 connected to the upper conduit-connection tube 48 ofa filling device 49, shown in detail in FIGURES 1 and 2.

Filling device 49 comprises an upper chamber element 50 and'a tubularlower chamber element 51 having a tapered. top end portion 52 adapted tobe sealingly and detachably secured in the downwardly flaring lower endportion 53 of upper chamber element 50. Chamber eletion 55 adapted'tosupportingly receivethe end of the calibrated tube portion .56 ofjthepenetrometer 57, as

Integrally formed with thebottom of the conical member'55 anddependingaxially therefrom is a conduit 55" provided with a manually operatedcut-oflf valve 56,

leading to a spherical reservoir 57; integrally connected to the end ofthe conduit 55'. A pressure-equalizingconduit 58v connects reservoir 57'to a portion of tubular Chamber 51 is provided with a horizontallyextending conduit element 59 provided with a three-way stop cock.

'64}, formed with an atmospheric vent conduit 61 andanother conduit 62,.said stop cock being of conventional 4 construction. The'stopcock6ilisprovidedwith an' "operating' element 63"which maybe rotated torespective diiferent positionsin which the stop cock (1).seals'otf iconduit59, (2) connects conduit '59to conduit 62, or.(3)

- connectsconduit 591 to atmospheric vent conduit 61.

As shown in FIGURE 1, the downwardly flaring skirt member 5.3.is formedat its lower end with a peripheral f bead 6:3. Abovesaid head, the skirtmember-531s pro vided with respectiveupwardly-and ontwardly' projectingl 1 ugs. 61f; 6-1'. 'The upper portion of chamber 51-is5pro f videdwithrespective downwardly and outwardly extenda lugs 56 62 lq atedb w t emes6 611 R Pec tivelcoiled fastening springsfiia' are. detachably fastenedeir endst pairs of'lugs 61', 62". and engage o the spring 'acts to{retain the. skirt member "53injsealin' I lin up l. v

s rneter, as described in a e e the veri n f h s we, h'w e l .as showninFIGURE :1, whereby theztension lso'ta djustably: supportedaining?suitable hydraulic, Ike, theco'nduit being supply valve 28. Alsosupported on this bracket is another bottle adapted to contain mercury,said last-named bottle being located below the filling device 49 andbeing so arranged that the depending vertical portion 72 of the conduitelement 62may be at times engaged through the neck of the bottle intothe mercury contained therein, whereby mercury may be admitted intoconduit 59 and into the filling device, as will be presently described.

The chamber elements 59 and 51 are formed of suitable transparentmaterial, such as glass, or the like.

The penetrometer 57 comprises the calibrated glass stem 56, open at oneend 73 and formed at its other end with a flaring bell-shaped member 74having an outwardly projecting to'p flange 63' provided with a groundflat annular top surface 64'. A ground flat disc 65' is engaged on thetop surface 64', the contacting surfaces being preferably coated with alight film of sealing material, such asv silicon grease. A cylindricalmetal ring member 66 surrounds fiange 63' and disc 65" and is formedwith an inturned bottom flange 67 which underlies flange 63'. The upperportion of ring member 66' is formed with internal threads 68 with whichare threadably engaged the external threads 69 of an annular clampingring 7t). An O-ring 71 of resilient deformable material, such as rubber,or the like, is engaged between the bottom end of ring 70 and theperipheral margin otdisc 65. Ring 70' is provided with a serrated topflange 79' which is substantially equal in outside diameter to the ringmember es, whose outside surface is similarly serrated.

The penetrometer stem is extended upwardly inside member 74, as shown at'72, so that it terminates a very short distance below the cover disc65', and is bevelled at its top end, as shown at 73. Thus, thereisidefined an annular space 74' around the extension 72, adapted toreceive the-material under test, for example, powdered material 75. Theopen end of extension 72' is above the surface of the sample 75' whenthe penetrometer is held in its customary upright position duringloading of the test sample in annular space 74, thus preventing thesample from sliding down the capillarybore 76. When the mercury rises inthis annular space 74 it floats the sample up to the top of the space;but since the mercury is flowing into the space via the open end ofextension 72', the sample cannot escape down the bore.

As is fully described in U.S. Patent No. 2,886,964, the

bottom member 31 of'pressure vessel 32 is formed with an internal cavityadapted to receivethe sample-containing bulb portion of the penetrometerwhen the penetrometer is in its working position (inverted as comparedwith the position thereof shown in FIGURE 1), and the pressure vessel 32is provided with a neck portion 81 having an internal bore of sufiicientsize to freely receive and ver tically support the penetrometer stem 56therein. The calibated stem of the penetrometer is visible through avertical transparent window provided inthe observation chamber 86.

In determining the pore sizes and volumes of a material, a weighedsample 75, of known volume or density,-ofi

the material is placed in thepenetromcter sample space 74 and said spaceis sealed by fastening the cover disc' 65' I'COILZIHd securing same onthe sealing surface 64- by means of the elements 66', 7d and 717,-asshown in FIGURE 3. The penetrometer 57 is-then placed, stem down, in thefilling device 49, Which is' then-closed, as shcwnin FIGURE '1, and iscorinectedno thevacuurn pump by the conduit 7 engaged on the' tub eelement; d8, .as'abovedescribed. i

p it The mercury bottle is .thenclamped position with the. mercuryfilling tube '1; well below-the su'rtacc. of

With vacuum valve t open andjthe device j the mercury,

draw mercury just beyond the stop cock into conduit 59, but not into thefilling chamber.

The filling chamber is then evacuated to a pressure below 100 microns,after which vacuum valve is closed.

Suflicient mercury to fill the penetrometer 57 is then admitted into thefilling device by means of stop cock 60. At this time the valve 56' isclosed, so that the mercury accumulates around the bottom end of stem 56in conical portion 55. i

The stop cock 6% is then carefully manipulated to admit air into thefilling device, forcing the mercury into the penetronieter, the stopcock 66 being closed at an air pressure in the filling chambersufiicientto completely fill the penetrometer, the value of said pressure beingindicated on gauge 21.

Following this, valve 56 may be opened to allow the excess mercury todrain into bulb 57, whereby the calibrations on the end of stem 56 maybe observcd for subsequent changes in the air pressure in the fillingchamber, with the apparatus in the position of FIGURE 1.

Thus, stop cock 6:) may be further manipulated to allow the air pressurein the filling chamber to increase, whereby the mercuryy in thepenetrometer bore will be forced upwardly in accordance with thepenetration of the mercury into the sample 75 as the air pressureincreases.

The above procedure allows the porosity data for the sample material tobe obtained at the large pore end of the spectrum, namely, the dataderived from the displacement of the end of the mercury column relativeto the calibrations on stem 56 as air is admitted to increase thepressure in the filling device in steps up to and including atmosphericpressure. r

After this preliminary data has been obtained, the filling device 49 iscarefully nnfastened fromits clamps and inverted, Ibeing refastened toits clamps in inverted position. The drop in level of the mercurycolumnin stem 56, corresponding to the volume of pores entered at thispressure, is then noted, said pressure being the sum of the pressure dueto the height of mercury above; the sample (1 inch of mercury=0.492pound per square inch gauge) and the indicated absolutepres'sure(atmospheric pressure). p i

The penetrometer 57 is then carefully removed from the filling device 49and is placed in the pressure vessel 32 for the continuationof the test,as described in U.S.

Patent bio-2,886,964. Thus, the penetrometer is in serted in thepressure vessel with its bulb portion housed in the member 31 and thecalibrations on the stem 56 facing outwardly and visible through thetransparent Window of observation section 86. The hydraulic fluid bottle7 (connected to conduit 34 through valve 28) is then raised to anelevated position such that liquid emerges from the bleeder valve 90,and is secured in said position, the

' jbleederwalve 90 being then closed. Valve 28 is'then closed; and thepressure in chamber 32 is then raised by rotating the handle 27 of thepressure generator 24, the pore volumes and pore diameters (as relatedto gauge pressures) being noted from the mercury column in stem 56, atappropriate intervals. Since stem Si t-is open at 'its top end, thepressure'in chainbert32 is applied" to the mercury column in" said sternandgtof the mercury in space 74', causing the height of said mercurycolumn to change withthe variations in pressure.- i i cock" its closed:to ace ates er and conduit 62;- the vac uum pu'mp is started.ilhestock' cock is then'care-v fullyfimanipulated by means of its value;handlef63 to.

' {When a. pressure of about 250p'ounds per square inch is. reached,valve 42 is'closed, the-higher=pressures being U- When the pore sizespectrurn'readingis have been pb- ,taincdiover.theLdesired pressurejrange,=fthej presiiur'e :is relieved 'byrbacking ofl.the pressure.generator ioperatirig screw slightly Valve. '28, hl'eeder valve sc amvalve 42 are then opened..-; 1The.hydraulicfluid"-@supply bottle is thenlowered toga' position below the top rim of them is her 31, allowingttheinstrument,to. drain."-- The pressure vessel fiz is their opened and thepenetrorrieter} 57 it;

sprees? removed, whereby the apparatus isreadyfor another determination.

While a specific embodiment of an improved apparatus for measuring thepore sizes and volumes of pores in material has been disclosed in theforegoing description, it will be understood that various modificationswithin the spirit of the invention may occur to those skilled in theart. Therefore it is intended that no limitations be placed on theinvention except as defined by the scope of the appended claims.

What is claimed is:

1. In a porosirneter, a penetrometer filling device comprising anelongated chamber adapted to receive a penetrometer in an uprightposition therein, a first conduit element communicatively connected tosaid chamber and adapted to be connected to a vacuum pump, a secondconduit element communicatively connected to said chamher and adapted tobe immersed in a quantity of filling liquid, air vent conduit means,valve means interconnecting said second conduit element, said air ventconduit means and said chamber and being formed and arranged toselectively control communication between said air vent conduit meansand said chamber and between said econd conduit element and saidchamber, a convergent end wall portion in said chamber supportinglyengage able with the open end of a penetrometer disposed in uprightposition in the chamber, a reservoir bulb subjacent said convergent endWall portion, conduit means communicatively connecting said bulb to thebottom of said end wall portion, and a cut-off valve in said lastnamedconduit means.

2. In a porosimeter, a penetrometer filling device comprising anelongated chamber adapted to receive a penetrometer in an uprightposition therein, a first conduit element communicatively connected tosaid chamber and adapted to be connected to a vacuum pump, a secondconduit element communicatively connected to said chamber and adapted tobe immersed in a quantity of filling liquid, air vent conduit means,valve means interconnecting said second conduit element, said air ventconduit means and said chamber and being formed and arranged toselectively control communication between said air vent conduit meansand said chamber and between said second conduit element and saidchamber, a convergent end wall portion in said chamber engageable withthe open end of a penetrometer disposed in upright position in thechamber, a reservoir bulb subjacent said convergent end wall portion,conduit means communicatively connecting said bulb to the bottom of saidend wall portion, a cutofl valve in said last-named conduit means, andfurther conduit means communicatively connecting said bulb to a point insaid chamber spaced a substantial distance above said convergent endwall portion.

3. In a porosimeter, a penetrometer filling device comprising anelongated chamber adapted to receive a penetrometer in an uprightposition therein, a first conduit element communicatively connected tothe upper portion of said chamber and adapted to be connected to avacuum pump, a second conduit element communicatively connected to theintermediate portion of said chamber and adapted to be immersed in aquantity of filling liquid, air vent conduit means, valve meansinterconnecting said second conduit element, said air vent conduit meansand said chamber and being formed and arranged to selectively controlcommunication between said air vent conduit means and said chamber andbetween said second conduit element and said chamber, a restriction insaid chamber adjacent the bottom end thereof and below the connection ofsaid second conduit element to the chamber, defining a reservoir bulb atsaid bottom end ti and defining a convergent wall portion above saidreservoir bulb adapted to supportingly engage the open end of apenetrometer disposed in said chamber, and a manually controlled valvemounted in said restriction.

4. In a porosimeter, a penetrometer filling device comprising anelongated chamber adapted to receive a penetrometer in an uprightposition therein, a first conduit element communicatively connected tothe upper portion of said chamber and adapted to be connected to avacuum pump, a second conduit element communicatively connected to theintermediate portion of said chamber and adapted to be immersed in aquantity of filling liquid, air vent conduit means, valve meansinterconnecting said second conduit element, said air vent conduit meansand said chamber and being formed and arranged to selectively controlcommunication between said air vent conduit means and said chamber andbetween said second conduit element and said chamber, a restriction insaid chamber adjacent the bottom end thereof and below the connection ofsaid second conduit element to the chamber, defining a reservoir bulb atsaid bottom end and defining a convergent wall portion above saidreservoir bulb adapted to supportingly engage the open end of apenetrometer disposed in said chamber, a manually controlled valvemounted in said restriction, and conduit means communicativelyconnecting said reservoir bulb to a point in said chamber spaced asubstantial distance above said restriction.

5. The structure of claim 4, and wherein said point is located betweensaid secondconduit element and said restriction.

6. In a porosimeter, a penetrometer filling device comprising anelongated chamber adapted to receive a penetrometer in an uprightposition therein, a first conduit element communicatively connected tothe top end portion of said chamber and adapted to be connected to avacuum pump, a second conduit element communicativly connected to theintermediate portion of said chamber and having an end portion extendingsubstantially parallel to said chamber and adapted to be immersed in aquantity of filling liquid, air vent conduit means, valve meansinterconnecting said second conduit element,

said air vent conduit means and said chamber and being formed andarranged to selectively control communication between said air ventconduit means and said chamber and between said second conduit elementand said chamber, a restriction in said chamber adjacent the bottom endportion thereof defining a reservoir bulb at the lower side of saidrestriction and defining a convergent wall portion above said reservoirbulb adapted to supportingly engage the open end of a penetrometerdisposed in said chamber, a manually controlled valve mounted in saidrestriction, and conduit means communicatively connecting said reservoirbulb to a point in said chamber spaced a substantial distance above saidrestriction.

References Cited in the file of this patent UNITED STATES PATENTS791,480 Maynard June 6, 1905 2,158,102 Betzold et al. May 16, 19392,369,591 Marden et al. Feb. 13, 1945 2,495,905 Pogue Jan. 31, 1950 v2,527,849 Ranney Oct. 31, 1950 2,641,924 Reichertz June 16, 19532,676,485 Morgan Apr. 27, 1954 2,696,937 Johnson et a1. Dec. 14, 19542,862,307 Bloomer et al. Dec. 2, 1958 2,886,964 Shapiro et a1. May 19,1959

1. IN A POROSIMETER, A PENETROMETER FILLING DEVICE COMPRISING ANELONGATED CHAMBER ADAPTED TO RECEIVE A PENETROMETER IN AN UPRIGHTPOSITION THEREIN, A FIRST CONDUIT ELEMENT COMMUNICATIVELY CONNECTED TOSAID CHAMBER AND ADAPTED TO BE CONNECTED TO A VACUUM PUMP, A SECONDCONDUIT ELEMENT COMMUNICATIVELY CONNECTED TO SAID CHAMBER AND ADAPTED TOBE IMMERSED IN A QUANTITY OF FILLING LIQUID, AIR VENT CONDUIT MEANS,VALVE MEANS INTERCONNECTING SAID SECOND CONDUIT ELEMENT, SAID AIR VENTCONDUIT MEANS AND SAID CHAMBER AND BEING FORMED AND ARRANGED TOSELECTIVELY CONTROL COMMUNICATION BETWEEN SAID AIR VENT CONDUIT MEANSAND SAID CHAMBER AND BETWEEN SAID SECOND CONDUIT ELEMENT AND SAIDCHAMBER, A CONVERGENT END WALL PORTION IN SAID CHAMBER SUPPORTINGLYENGAGEABLE WITH THE OPEN END OF A PENETROMETER DISPOSED IN UPRIGHTPOSITION IN THE CHAMBER, A RESERVOIR BULB SUBJACENT SAID CONVERGENT ENDWALL PORTION, CONDUIT MEANS